Here, a simple method is used for the preparation of calcium alginate-activated carbon composite beads (Alg-ACBDs). These beads were introduced into different metal salt solutions for decoration with single metal nanoparticle (M-0) and double metal nanoparticles (M-0-M-0). The prepared M-0/Alg-ACBDs catalysts, such as, Cu-0/Alg-ACBDs, Ag-0/Alg-ACBDs, Fe-0/Alg-ACBDs, Cu-0-Ag-0/Alg-ACBDs, and Fe-0-Cu-0/Alg-ACBDs were evaluated against NaBH4 methanolysis. In addition, different surfactants, such as, brij-56, pluronic F-127, and urea (Co (NH2)(2)), different amount of NaBH4, catalyst, and temperature effect was also investigated for higher H-2 generation from NaBH4 methanolysis. Similarly, the synthesized catalysts were used for the reduction of different nitrophenols (NPs) and dyes. The Fe-0-Cu-0/Alg-ACBDs catalyst efficiently catalyzed the reduction reaction of 4-NP and methyl orange (MO) and both were studied in detail. The corresponding reduction rate of 4-NP and MO was observed as 1.829 and 1.163 min(-1), respectively. Moreover, the recyclability of the catalyst was investigated for 4-NP and H-2 generation, where no decrease in the reduction percentage of 4-NP was recorded, while reduction in their catalytic rates was observed.